#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:36:53 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178907 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/36/4113615.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4113615
loop_
_publ_author_name
'Joshua S. Figueroa'
'Christopher C. Cummins'
_publ_section_title
;
 The Niobaziridine-Hydride Functional Group: Synthesis and Divergent
 Reactivity
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4020
_journal_page_last               4021
_journal_paper_doi               10.1021/ja028446y
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C39 H60 N3 Nb'
_chemical_formula_weight         663.81
_chemical_name_common            Nb(H)(tBu(H)C=NAr)(N[Np]Ar)2
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.0920(10)
_cell_angle_beta                 84.3140(10)
_cell_angle_gamma                66.6050(10)
_cell_formula_units_Z            2
_cell_length_a                   11.0193(7)
_cell_length_b                   11.2042(7)
_cell_length_c                   17.2591(12)
_cell_measurement_reflns_used    121
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      23.28
_cell_measurement_theta_min      2.37
_cell_volume                     1919.7(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7646
_diffrn_reflns_theta_full        23.28
_diffrn_reflns_theta_max         23.28
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    0.341
_exptl_absorpt_correction_T_max  0.9165
_exptl_absorpt_correction_T_min  0.8163
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.821
_refine_diff_density_min         -1.165
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         5394
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0765P)²+1.1306P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1076
_refine_ls_wR_factor_ref         0.1092
_reflns_number_gt                5137
_reflns_number_total             5394
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja028446ysi20030122_052029_1.cif
_cod_data_source_block           01159m
_cod_database_code               4113615
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Nb Nb 0.28128(2) 1.37095(2) 0.215397(12) 0.02611(13) Uani 1 1 d .
N2 N 0.3026(2) 1.2268(2) 0.15618(13) 0.0295(5) Uani 1 1 d .
N3 N 0.4258(2) 1.4144(2) 0.15822(13) 0.0288(5) Uani 1 1 d .
C21 C 0.2976(3) 1.1166(3) 0.21089(16) 0.0305(6) Uani 1 1 d .
C37 C 0.3350(3) 1.5398(3) 0.17082(17) 0.0291(6) Uani 1 1 d .
C38 C 0.2795(3) 1.6498(3) 0.10073(17) 0.0326(6) Uani 1 1 d .
N1 N 0.3289(3) 1.3233(3) 0.33019(14) 0.0367(6) Uani 1 1 d .
C34 C 0.8345(3) 1.2432(3) 0.18438(19) 0.0401(7) Uani 1 1 d .
C33 C 0.7675(3) 1.1657(3) 0.17297(19) 0.0405(7) Uani 1 1 d .
C35 C 0.7690(3) 1.3764(3) 0.18652(17) 0.0350(7) Uani 1 1 d .
C27 C 0.3504(3) 1.2070(3) 0.07503(17) 0.0322(6) Uani 1 1 d .
C31 C 0.5638(3) 1.3587(3) 0.16496(15) 0.0281(6) Uani 1 1 d .
C26 C 0.4023(3) 0.9932(3) 0.21970(18) 0.0368(7) Uani 1 1 d .
C36 C 0.6338(3) 1.4340(3) 0.17530(16) 0.0313(6) Uani 1 1 d .
C25 C 0.3945(4) 0.8889(3) 0.27404(18) 0.0450(8) Uani 1 1 d .
C351 C 0.8422(4) 1.4582(4) 0.2015(3) 0.0488(8) Uani 1 1 d .
C211 C 0.1292(4) 1.3325(4) 0.0113(3) 0.0579(10) Uani 1 1 d .
C311 C 0.3845(4) 1.7064(4) 0.0680(2) 0.0428(8) Uani 1 1 d .
C310 C 0.1571(3) 1.7584(3) 0.1296(2) 0.0453(8) Uani 1 1 d .
C32 C 0.6321(3) 1.2242(3) 0.16387(17) 0.0337(6) Uani 1 1 d .
C39 C 0.2429(4) 1.5993(4) 0.0346(2) 0.0412(7) Uani 1 1 d .
C22 C 0.1852(3) 1.1336(3) 0.25964(17) 0.0358(7) Uani 1 1 d .
C16 C 0.1449(4) 1.2962(4) 0.42021(19) 0.0479(8) Uani 1 1 d .
C28 C 0.2496(3) 1.2043(3) 0.02023(17) 0.0348(6) Uani 1 1 d .
C23 C 0.1751(4) 1.0295(3) 0.31515(18) 0.0441(8) Uani 1 1 d .
C210 C 0.3193(4) 1.1866(5) -0.0601(2) 0.0510(9) Uani 1 1 d .
C17 C 0.4370(4) 1.2062(4) 0.3659(2) 0.0487(8) Uani 1 1 d .
C12 C 0.1216(3) 1.5004(3) 0.33425(18) 0.0418(8) Uani 1 1 d .
C24 C 0.2807(4) 0.9080(4) 0.3210(2) 0.0509(9) Uani 1 1 d .
C11 C 0.2013(3) 1.3705(3) 0.36506(16) 0.0384(7) Uani 1 1 d .
C13 C -0.0135(4) 1.5552(4) 0.3546(2) 0.0524(9) Uani 1 1 d .
C231 C 0.0492(5) 1.0491(6) 0.3636(3) 0.0649(11) Uani 1 1 d .
C29 C 0.2062(6) 1.0896(5) 0.0499(3) 0.0615(11) Uani 1 1 d .
C15 C 0.0135(4) 1.3514(4) 0.4435(2) 0.0539(9) Uani 1 1 d .
C18 C 0.5218(4) 1.2328(5) 0.4214(2) 0.0662(12) Uani 1 1 d .
C14 C -0.0643(4) 1.4795(5) 0.4090(2) 0.0586(10) Uani 1 1 d .
C331 C 0.8408(4) 1.0210(4) 0.1700(3) 0.0695(12) Uani 1 1 d .
H33A H 0.7780 0.9827 0.1617 0.104 Uiso 1 1 calc R
H33B H 0.8856 0.9765 0.2199 0.104 Uiso 1 1 calc R
H33C H 0.9064 1.0096 0.1264 0.104 Uiso 1 1 calc R
C251 C 0.5090(6) 0.7567(4) 0.2823(3) 0.0662(12) Uani 1 1 d .
C131 C -0.0960(5) 1.6926(5) 0.3178(3) 0.0713(12) Uani 1 1 d .
C111 C 0.5770(7) 1.3309(8) 0.3782(3) 0.0791(16) Uani 1 1 d .
C110 C 0.6357(7) 1.1009(10) 0.4468(5) 0.114(3) Uani 1 1 d .
C151 C -0.0473(6) 1.2748(7) 0.5049(3) 0.0733(14) Uani 1 1 d .
C19 C 0.4395(7) 1.2831(11) 0.4933(3) 0.106(3) Uani 1 1 d .
H36A H 0.591(3) 1.515(3) 0.1804(17) 0.024(7) Uiso 1 1 d .
H37A H 0.356(3) 1.570(3) 0.2143(17) 0.021(7) Uiso 1 1 d .
H22A H 0.108(3) 1.217(3) 0.2513(17) 0.026(7) Uiso 1 1 d .
H32A H 0.587(3) 1.173(3) 0.1552(17) 0.029(7) Uiso 1 1 d .
H34A H 0.921(4) 1.210(3) 0.1886(19) 0.037(8) Uiso 1 1 d .
H27B H 0.425(3) 1.133(3) 0.0761(18) 0.031(8) Uiso 1 1 d .
H27A H 0.373(3) 1.277(3) 0.0551(18) 0.029(8) Uiso 1 1 d .
H26A H 0.482(4) 0.980(3) 0.186(2) 0.040(9) Uiso 1 1 d .
H1 H 0.139(3) 1.473(3) 0.185(2) 0.047(9) Uiso 1 1 d .
H17B H 0.403(4) 1.142(4) 0.393(2) 0.055(11) Uiso 1 1 d .
H16A H 0.201(4) 1.201(4) 0.437(2) 0.064(12) Uiso 1 1 d .
H14A H -0.147(4) 1.518(4) 0.421(2) 0.054(11) Uiso 1 1 d .
H21A H 0.395(5) 1.099(5) -0.056(3) 0.076(13) Uiso 1 1 d .
H17A H 0.494(4) 1.169(4) 0.323(2) 0.057(11) Uiso 1 1 d .
H39A H 0.201(4) 1.667(4) -0.004(3) 0.064(12) Uiso 1 1 d .
H31D H 0.352(3) 1.772(3) 0.026(2) 0.035(8) Uiso 1 1 d .
H39B H 0.318(4) 1.531(4) 0.016(2) 0.042(9) Uiso 1 1 d .
H12A H 0.160(3) 1.555(3) 0.309(2) 0.038(9) Uiso 1 1 d .
H39C H 0.174(4) 1.567(3) 0.051(2) 0.041(9) Uiso 1 1 d .
H31A H 0.088(4) 1.725(4) 0.148(2) 0.051(10) Uiso 1 1 d .
H31E H 0.466(4) 1.638(4) 0.054(2) 0.044(9) Uiso 1 1 d .
H35A H 0.793(4) 1.554(5) 0.193(3) 0.071(13) Uiso 1 1 d .
H31F H 0.410(4) 1.737(5) 0.113(3) 0.075(13) Uiso 1 1 d .
H31C H 0.181(4) 1.796(4) 0.171(2) 0.056(11) Uiso 1 1 d .
H21D H 0.073(4) 1.335(4) -0.022(3) 0.066(12) Uiso 1 1 d .
H31B H 0.131(4) 1.824(5) 0.092(3) 0.063(12) Uiso 1 1 d .
H21B H 0.353(4) 1.252(4) -0.082(2) 0.059(11) Uiso 1 1 d .
H35B H 0.881(4) 1.430(4) 0.250(3) 0.054(11) Uiso 1 1 d .
H21E H 0.156(5) 1.409(5) -0.015(3) 0.084(15) Uiso 1 1 d .
H21C H 0.257(4) 1.184(4) -0.097(2) 0.055(10) Uiso 1 1 d .
H23A H -0.008(5) 1.136(5) 0.368(3) 0.072(14) Uiso 1 1 d .
H23B H 0.015(5) 1.006(5) 0.351(3) 0.081(17) Uiso 1 1 d .
H13A H -0.058(5) 1.759(5) 0.322(3) 0.088(16) Uiso 1 1 d .
H13B H -0.172(6) 1.735(5) 0.341(3) 0.094(17) Uiso 1 1 d .
H25A H 0.562(4) 0.752(4) 0.325(3) 0.065(12) Uiso 1 1 d .
H11D H 0.504(5) 1.415(5) 0.365(3) 0.066(14) Uiso 1 1 d .
H21F H 0.086(4) 1.347(4) 0.062(3) 0.065(12) Uiso 1 1 d .
H19A H 0.374(5) 1.365(5) 0.481(3) 0.067(16) Uiso 1 1 d .
H11E H 0.629(5) 1.352(4) 0.410(3) 0.073(13) Uiso 1 1 d .
H23C H 0.072(5) 1.019(5) 0.415(4) 0.092(17) Uiso 1 1 d .
H24A H 0.272(4) 0.839(5) 0.354(3) 0.075(14) Uiso 1 1 d .
H11A H 0.677(7) 1.110(7) 0.483(4) 0.12(2) Uiso 1 1 d .
H29A H 0.157(4) 1.103(4) 0.099(3) 0.068(12) Uiso 1 1 d .
H15A H -0.088(5) 1.319(5) 0.550(3) 0.093(16) Uiso 1 1 d .
H19C H 0.491(5) 1.297(5) 0.527(3) 0.090(15) Uiso 1 1 d .
H15B H 0.016(6) 1.193(7) 0.530(4) 0.11(2) Uiso 1 1 d .
H11F H 0.621(7) 1.298(7) 0.345(4) 0.12(3) Uiso 1 1 d .
H25B H 0.563(6) 0.741(6) 0.231(4) 0.112(19) Uiso 1 1 d .
H35C H 0.913(6) 1.447(5) 0.175(3) 0.097(18) Uiso 1 1 d .
H19B H 0.396(6) 1.225(6) 0.524(4) 0.11(2) Uiso 1 1 d .
H25C H 0.476(5) 0.696(6) 0.298(3) 0.095(18) Uiso 1 1 d .
H29B H 0.148(4) 1.086(4) 0.013(3) 0.063(11) Uiso 1 1 d .
H15C H -0.112(5) 1.268(5) 0.480(3) 0.074(14) Uiso 1 1 d .
H29C H 0.280(5) 1.013(5) 0.053(3) 0.074(15) Uiso 1 1 d .
H13C H -0.121(6) 1.696(6) 0.271(4) 0.10(2) Uiso 1 1 d .
H11B H 0.606(8) 1.034(8) 0.463(5) 0.15(3) Uiso 1 1 d .
H11C H 0.693(7) 1.064(7) 0.401(4) 0.12(2) Uiso 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
H1 Nb N3 112.5(12)
H1 Nb N2 98.9(12)
N3 Nb N2 95.18(9)
H1 Nb N1 122.7(12)
N3 Nb N1 105.68(10)
N2 Nb N1 118.72(10)
H1 Nb C37 82.4(13)
N3 Nb C37 39.19(10)
N2 Nb C37 125.66(10)
N1 Nb C37 104.35(10)
H1 Nb C11 92.0(12)
N3 Nb C11 130.77(9)
N2 Nb C11 123.49(10)
N1 Nb C11 31.67(10)
C37 Nb C11 110.66(10)
C21 N2 C27 118.1(2)
C21 N2 Nb 108.79(17)
C27 N2 Nb 131.34(19)
C31 N3 C37 129.3(2)
C31 N3 Nb 133.49(19)
C37 N3 Nb 78.76(15)
C22 C21 C26 118.7(3)
C22 C21 N2 118.5(3)
C26 C21 N2 122.8(3)
N3 C37 C38 120.3(2)
N3 C37 Nb 62.05(14)
C38 C37 Nb 128.86(19)
C39 C38 C310 109.9(3)
C39 C38 C37 111.4(2)
C310 C38 C37 108.3(3)
C39 C38 C311 108.1(3)
C310 C38 C311 109.6(3)
C37 C38 C311 109.6(2)
C11 N1 C17 123.1(3)
C11 N1 Nb 99.57(18)
C17 N1 Nb 126.2(2)
C35 C34 C33 121.6(3)
C32 C33 C34 118.8(3)
C32 C33 C331 120.4(3)
C34 C33 C331 120.9(3)
C34 C35 C36 118.7(3)
C34 C35 C351 121.0(3)
C36 C35 C351 120.2(3)
N2 C27 C28 115.9(2)
C36 C31 C32 119.1(3)
C36 C31 N3 121.5(3)
C32 C31 N3 119.4(2)
C25 C26 C21 121.2(3)
C35 C36 C31 120.9(3)
C26 C25 C24 119.0(3)
C26 C25 C251 120.0(4)
C24 C25 C251 121.0(4)
C33 C32 C31 120.8(3)
C21 C22 C23 121.2(3)
C15 C16 C11 120.3(4)
C211 C28 C210 108.9(3)
C211 C28 C29 109.4(4)
C210 C28 C29 108.9(3)
C211 C28 C27 111.2(3)
C210 C28 C27 106.4(3)
C29 C28 C27 111.8(3)
C24 C23 C22 118.2(3)
C24 C23 C231 121.9(4)
C22 C23 C231 119.8(4)
N1 C17 C18 114.5(3)
C11 C12 C13 121.4(3)
C25 C24 C23 121.8(3)
C12 C11 C16 118.7(3)
C12 C11 N1 114.7(3)
C16 C11 N1 126.3(3)
C12 C11 Nb 80.96(18)
C16 C11 Nb 135.5(2)
N1 C11 Nb 48.76(13)
C14 C13 C12 117.9(4)
C14 C13 C131 122.5(4)
C12 C13 C131 119.5(4)
C16 C15 C14 119.4(3)
C16 C15 C151 121.0(4)
C14 C15 C151 119.7(4)
C111 C18 C19 110.4(6)
C111 C18 C110 109.4(5)
C19 C18 C110 110.1(6)
C111 C18 C17 110.3(3)
C19 C18 C17 110.2(4)
C110 C18 C17 106.4(5)
C13 C14 C15 122.2(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Nb H1 1.60(3)
Nb N3 1.967(2)
Nb N2 1.996(2)
Nb N1 2.017(2)
Nb C37 2.183(3)
Nb C11 2.645(3)
N2 C21 1.422(4)
N2 C27 1.472(4)
N3 C31 1.404(4)
N3 C37 1.407(4)
C21 C22 1.394(4)
C21 C26 1.398(4)
C37 C38 1.530(4)
C38 C39 1.517(4)
C38 C310 1.530(4)
C38 C311 1.541(4)
N1 C11 1.408(4)
N1 C17 1.455(4)
C34 C35 1.382(5)
C34 C33 1.393(5)
C33 C32 1.382(4)
C33 C331 1.506(5)
C35 C36 1.386(4)
C35 C351 1.507(5)
C27 C28 1.541(4)
C31 C36 1.392(4)
C31 C32 1.394(4)
C26 C25 1.380(5)
C25 C24 1.388(5)
C25 C251 1.509(5)
C211 C28 1.514(5)
C22 C23 1.397(5)
C16 C15 1.381(5)
C16 C11 1.407(5)
C28 C210 1.524(5)
C28 C29 1.527(5)
C23 C24 1.389(5)
C23 C231 1.506(6)
C17 C18 1.545(5)
C12 C11 1.399(5)
C12 C13 1.403(5)
C13 C14 1.373(6)
C13 C131 1.495(6)
C15 C14 1.396(6)
C15 C151 1.510(6)
C18 C111 1.505(7)
C18 C19 1.522(7)
C18 C110 1.530(9)
